関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 反応物 | 2,3-Dichloro-5-hydroxypyridine | HCID 14391672 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,3-Dichloro-5-(2,2-diethoxyethoxy)pyridine | HCID 86645896 | 88.4% |
反応手順
Bromoacetaldehyde diethyl acetal (2.74 ml, 18.3 mmol) and cesium carbonate (9.93 g, 30.5 mmol) were added to an N,N-dimethylacetamide solution (10 ml) of 5,6-dichloropyridin-3-ol (1.0 g, 6.10 mmol), and stirred under a nitrogen atmosphere at 100° C. for 16 hours. Saline solution and ethyl acetate were added to the reaction solution, the organic layer was washed with water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (Biotage, hexane:ethyl acetate=11:1 to 9:1) to obtain 2,3-dichloro-5-(2,2-diethoxyethoxy)pyridine (1.51 g, yield: 88%) as an orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846700B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-499267f0d56448ea863eca0a72cb2f61 |
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| 出典メモ | uspto-grants-2014_09 |
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